EP3325196A1 - Plasma atomization metal powder manufacturing processes and systems therefore - Google Patents
Plasma atomization metal powder manufacturing processes and systems thereforeInfo
- Publication number
- EP3325196A1 EP3325196A1 EP16826954.6A EP16826954A EP3325196A1 EP 3325196 A1 EP3325196 A1 EP 3325196A1 EP 16826954 A EP16826954 A EP 16826954A EP 3325196 A1 EP3325196 A1 EP 3325196A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- source
- manufacturing process
- plasma
- metal
- heated
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 347
- 239000002184 metal Substances 0.000 title claims abstract description 347
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 114
- 238000000889 atomisation Methods 0.000 title claims abstract description 112
- 239000000843 powder Substances 0.000 title claims abstract description 97
- 238000009826 distribution Methods 0.000 claims abstract description 37
- 239000002245 particle Substances 0.000 claims abstract description 35
- 238000011144 upstream manufacturing Methods 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims description 42
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 32
- 238000001816 cooling Methods 0.000 claims description 20
- 239000010936 titanium Substances 0.000 claims description 17
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 14
- 238000010891 electric arc Methods 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 13
- 229910052719 titanium Inorganic materials 0.000 claims description 13
- 229910052726 zirconium Inorganic materials 0.000 claims description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 12
- 150000002739 metals Chemical class 0.000 claims description 12
- 238000006073 displacement reaction Methods 0.000 claims description 11
- 230000006698 induction Effects 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 11
- 229910000838 Al alloy Inorganic materials 0.000 claims description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 10
- 229910001093 Zr alloy Inorganic materials 0.000 claims description 10
- 239000000155 melt Substances 0.000 claims description 10
- 229910000601 superalloy Inorganic materials 0.000 claims description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 7
- 229910052750 molybdenum Inorganic materials 0.000 claims description 7
- 239000011733 molybdenum Substances 0.000 claims description 7
- 229910052758 niobium Inorganic materials 0.000 claims description 7
- 239000010955 niobium Substances 0.000 claims description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 7
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052721 tungsten Inorganic materials 0.000 claims description 7
- 239000010937 tungsten Substances 0.000 claims description 7
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 6
- 229910001182 Mo alloy Inorganic materials 0.000 claims description 6
- 229910001257 Nb alloy Inorganic materials 0.000 claims description 6
- 229910001080 W alloy Inorganic materials 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 239000011777 magnesium Substances 0.000 claims description 6
- 229910017052 cobalt Inorganic materials 0.000 claims description 5
- 239000010941 cobalt Substances 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 5
- 238000011109 contamination Methods 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 239000012777 electrically insulating material Substances 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 229910052707 ruthenium Inorganic materials 0.000 claims description 4
- 238000000365 skull melting Methods 0.000 claims description 4
- 229910021324 titanium aluminide Inorganic materials 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims 2
- 239000000919 ceramic Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 38
- 239000007789 gas Substances 0.000 description 45
- 238000001637 plasma atomic emission spectroscopy Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- 239000011261 inert gas Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 230000004927 fusion Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000002923 metal particle Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 239000002826 coolant Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003779 heat-resistant material Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 238000001746 injection moulding Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 238000010146 3D printing Methods 0.000 description 1
- 239000006091 Macor Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000000112 cooling gas Substances 0.000 description 1
- 239000000110 cooling liquid Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 238000010191 image analysis Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/0408—Light metal alloys
- C22C1/0416—Aluminium-based alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/045—Alloys based on refractory metals
- C22C1/0458—Alloys based on titanium, zirconium or hafnium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0836—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid with electric or magnetic field or induction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
- B22F2009/0892—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid casting nozzle; controlling metal stream in or after the casting nozzle
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2202/00—Treatment under specific physical conditions
- B22F2202/13—Use of plasma
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2304/00—Physical aspects of the powder
- B22F2304/10—Micron size particles, i.e. above 1 micrometer up to 500 micrometer
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Definitions
- the present disclosure relates to the field of production of spheroidal powders such as metal spheroidal powders. More particularly, it relates to methods and apparatuses for preparing metal powders by means of a plasma atomization process.
- the desired features of high quality reactive metal powders will be a combination of high sphericity, density, purity, flowability and low amount of gas entrapped porosities.
- Fine powders are useful for applications such as 3D printing, powder injection molding, hot isostatic pressing and coatings. Such fine powders are used in aerospace, biomedical and industrial fields of applications.
- typical process such as EIGA process, may require a very large quantity of atomizing gas in order to achieve the yield of 70% of particles having a size between 0-106 ⁇ .
- the Gas to Metal ratio in EIGA process can be as high as about 33. This may further increase production costs.
- a plasma atomization metal powder manufacturing process comprising: providing a heated metal source; and contacting said heated metal source with the plasma of at least one plasma source under conditions effective for causing atomization of said heated metal source.
- a plasma atomization metal powder manufacturing process comprising: providing a heated metal source; and contacting said heated metal source with the plasma of at least one plasma source under conditions effective for causing atomization of said heated metal source, thereby obtaining a raw metal powder having a 0-106 ⁇ particle size distribution yield of at least 80%, measured according to ASTM B214.
- a plasma atomization metal powder manufacturing process comprising providing a heated metal source, contacting said heated metal source with the plasma of at least one plasma source under conditions effective for causing atomization of said heated metal source, wherein said atomization is carried out by using a gas to metal ratio of less than about 20, thereby obtaining a raw metal powder having a 0- 106 ⁇ particle size distribution yield of at least 80%, measured according to ASTM B214.
- a plasma atomization metal powder manufacturing process comprising providing a heated metal source, contacting said heated metal source with the plasma of at least one plasma source under conditions effective for causing atomization of said heated metal source, wherein said atomization is carried out by using a gas to metal ratio of less than about 20, thereby obtaining a metal powder having a 0-106 ⁇ distribution of at least 80%.
- a plasma atomization manufacturing process comprising providing a heated metal source, aligning the heated metal source with the plasma of at least one plasma source, and contacting the heated metal source with the plasma of the least one plasma source under conditions effective for causing atomization of said heated metal source.
- a atomizing system comprising a feeder for feeding a metal source, at least one heating system for heating the metal source, at least one plasma source configured for contacting the metal source after heating with plasma under conditions effective for causing atomization of the heated metal source, and an alignment system positioned upstream of the at least one plasma source, the alignment system being adapted to adjust an orientation of the metal source relative to the at least one plasma source.
- FIG. 1 is a cross-sectional view of an atomizing system according to a first exemplary embodiment of the present disclosure
- Figure 2 is a schematic diagram of an aligning system of an atomizing system according to one exemplary embodiment of the present disclosure
- Figure 3 is a cross-sectional view of a guide of a guided atomizing system according to one exemplary embodiment of the present disclosure
- Figure 4 is a cross-sectional view of a guide having an induction heating element according to one exemplary embodiment of the present disclosure
- Figure 5 is a cross-sectional view of a guide having at an electrode heating element according to another exemplary embodiment of the present disclosure
- Figure 6 is a cross-sectional view of a guided atomizing system according to a first exemplary embodiment of the present disclosure
- Figure 7 is a cross-sectional view of a guided atomizing system according to a second exemplary embodiment of the present disclosure.
- Figure 8 is a cross-sectional view of a guided atomizing system according to a third exemplary embodiment of the present disclosure.
- Figure 9 is a SEM image at 250 times magnification of metal particles (Ti-6AI-4V) according to one example atomization process of the present disclosure
- Figure 10 is a SEM image at 500 times magnification of metal particles (Ti-6AI-4V) according to one example atomization process of the present disclosure.
- Figure 1 1 is a SEM image at 2000 times magnification of metal particles (Ti-6AI-4V) according to one example atomization process of the present disclosure.
- atomization zone refers to a zone in which the material is atomized into droplets of the material.
- the person skilled in the art would understand that the dimensions of the atomization zone will vary according to various parameters such as temperature of the atomizing means, velocity of the atomizing means, material in the atomizing means, power of the atomizing means, temperature of the material before entering in the atomization zone, nature of the material, dimensions of the material, electrical resistivity of the material etc.
- metal powder has a X-Y ⁇ particle size distribution yield of at least T %, measured according to ASTM B214
- metal powder having a 0-106 ⁇ particle size distribution yield of at least 80%, measured according to ASTM B214 refers to a metal powder in which at least 80 % of the obtained powder has a particle size distribution of about 0 to about 106 ⁇ . The value is measured according to ASTM B214 standard
- Gas to Metal ratio refers to the mass per unit of time (Kg/s) of gas injected for the mass rate (Kg/s) of metal source to the atomization zone.
- reactive metal powder refers to a metal powder that cannot be efficiently prepared via the classical gas atomization process in which close-coupled nozzle is used.
- a reactive metal powder can be a powder comprising at least one member chosen from one of titanium, titanium alloys, zirconium, zirconium alloys, magnesium, magnesium alloys, niobium, niobium alloys, aluminum, aluminum alloys, molybdenum, molybdenum alloys, tungsten, tungsten alloys, oxygen-reactive metals, and nitrogen-reactive metals.
- raw metal powder refers to a metal powder obtained directly from an atomization process without any post processing steps such as sieving or classification techniques.
- Various exemplary embodiments described herein provide a high yield of raw metal powder of a given distribution while keeping low production costs. Production costs are kept low by minimizing the waste and by reducing the gas flow (i.e. amount of gas) that is used in the atomization process.
- the gas to metal ratio according to methods and systems described herein is less than 30.
- a metal source is provided.
- the raw metal powder is to be formed from the atomization of this metal source.
- the metal source is preheated prior to entering in the atomization zone.
- the metal source has already been heated prior to being fed into an atomization zone. However, the metal source is further heated immediately upstream of the atomization zone so that the metal source reaches a sufficient temperature prior to being atomized. Having reached the sufficient temperature, the metal source is atomized by being contacted by plasma from at least one plasma source under conditions that are effective for causing atomization of the heated metal source.
- the raw material can be melted in a water-cooled crucible (skull melting).
- the metal source is then a melt stream that can be further heated and fed to the atomization zone to be contacted by the plasma from the at least one plasma source to be atomized.
- the metal source may be initially fed as a metal wire or metal rod.
- the metal wire or metal rod Prior to atomization, the metal wire or metal rod may be further heated by resistive heating, arc discharge, induction heating or any combination thereof. After being heated, the metal wire or metal rod is fed into the atomization zone to be contacted by the plasma from the at least one plasma source to be atomized.
- the temperature of the metal source prior to atomization can be close to the melting point of the material.
- the temperature can be about 75 % to about 1 10 % of the melting point temperature or about 85 % to about 95 % of the melting point temperature.
- the high yield of fine powder is achieved for a low amount of very hot gas flow injected within the atomization zone. It will be appreciated that the injected gas will often be an inert gas. Reducing the amount of injected gas can significantly decrease production costs, especially the recycling gas costs.
- the plasma from the at least one plasma source must provide sufficient heating energy and momentum to the metal source during atomization.
- the plasma gas flow is typically more than 100 slm per torch, more preferably more than 150 slm for 3 convergent plasma torches for a mass feed rate of titanium of about 10 kg/h.
- the electrical power per torch is about 25 kW and more preferably about 30 kW and more.
- raw metal powder may be formed from atomizing the metal source while using a gas-to-metal ratio of less than about 20.
- raw metal powder may be formed from atomizing the metal source while using a gas-to-metal ratio of about 5 to about 15.
- raw metal powder may be formed from atomizing the metal source while using a gas-to-metal ratio of about 2 to about 10.
- raw metal powder may be formed from atomizing the metal source while using a gas-to-metal ratio of about 5 to about 10.
- raw metal powder may be formed from atomizing the metal source while using a gas-to-metal ratio of about 10 to about 20.
- raw metal powder may be formed from atomizing the metal source while using a gas-to-metal ratio of about 10 to about 15.
- the raw metal powder obtained from atomization has a 0-106 ⁇ particle size distribution yield of at least 80%.
- the raw metal powder obtained from atomization has 0-106 ⁇ particle size distribution yield of at least 85%.
- the raw metal powder obtained from atomization has a of 0-106 ⁇ particle size distribution yield of at least 90%.
- the raw metal powder obtained from atomization has a 0-75 ⁇ particle size distribution yield of at least 85%.
- the raw metal powder obtained from atomization has a 0-45 ⁇ particle size distribution yield of at least 50%.
- the raw metal powder obtained from atomization has a 0-45 ⁇ particle size distribution yield of at least 60%.
- the metal source fed into the atomization zone is appropriately positioned relative to the plasma and the at least one plasma source.
- the metal source fed into the atomization zone and the at least one plasma source is positioned relative to one another so that metal source contacts the plasma at an apex of the plasma source. This may be the geometric apex of the plasma source. It was observed that the apex of the plasma source corresponds to the region where the atomizing shearing forces of the plasma are the greatest.
- the proper relative positioning of the metal source within the atomization zone and the at least one plasma source may require the nozzle outlet of the plasma source to be placed in close proximity of the metal source in the atomization zone.
- the plasma source is positioned so that its nozzle outlet is within at most about 5 centimeters of the metal source.
- the plasma source is positioned so that its nozzle outlet is within at most about 3 centimeters of the metal source.
- the plasma source is positioned so that its nozzle outlet is within at most about 2.5 centimeters of the metal source.
- the plasma source is positioned so that its nozzle outlet is within at most about 2 centimeters of the metal source.
- the plasma source is positioned so that its nozzle outlet is within at most about 1 .9 centimeters of the metal source.
- the plasma source is positioned so that its nozzle outlet is within at most about 1 .75 centimeters of the metal source.
- the plasma source is positioned so that its nozzle outlet is within at most about 1 .5 centimeters of the metal source.
- the metal source is fed into the atomization zone as a vertical feed.
- This feed may be a melt stream, metal rod or metal wire.
- the at least one plasma source may be at least one plasma torch having at least one discrete nozzle. Where a plurality of discrete nozzles is provided, these nozzles may be positioned angularly about the metal source vertical feed. [0068] Alternatively, the at least one plasma source may include an annular nozzle extending around the metal source vertical feed.
- the at least one nozzle of the at least one plasma source may be angled downwardly.
- the at least one plasma source may emit plasma jets that are oriented at about 10° to about 60° relative to the vertical axis.
- the at least one plasma source may emit plasma jets that are oriented at about 20° to about 60° relative to the vertical axis.
- the at least one plasma source may emit plasma jets that are oriented at about 20° to about 50° relative to the vertical axis.
- the at least one plasma source may emit plasma jets that are oriented at about 20° to about 30° relative to the vertical axis.
- the at least one plasma source may emit plasma jets that are oriented at about 25° to about 35° relative to the vertical axis.
- the metal source fed into the atomization zone is aligned with the plasma of the at least one plasma source.
- the aligning may include adjusting the orientation of the metal source as it is being fed into the atomization zone. This adjustment seeks to maintain a desired positioning of the metal source relative to the at least one plasma source and/or the plasma from the at least one plasma source over time.
- the position of the metal source being fed into the atomization zone can spatially fluctuate over time. This spatial fluctuate may occur between separate atomization runs or within a single atomization run. Accordingly, the orientation of the metal source as it is being fed into the atomization zone may be adjusted prior to beginning an atomization run.
- the melt stream falling from a melted rod can move and not always contact the exact plasma jet apex (atomization point).
- the hot wire and small rod can bend and move away from the optimal atomization point.
- the orientation of the metal source as it is being fed into the atomization zone may be adjusted repeatedly during an ongoing atomization process.
- the adjustment of the orientation of the metal source may be carried out continuously or intermittently in order to maintain a desired alignment of the metal source with the plasma source and/or the plasma from the at least one plasma source.
- the orientation of the metal source being fed into the atomization zone may be visually monitored by a human operator.
- the operator may operate (manually or via inputting of a computerized command) an alignment-correcting mechanism so as to adjust orientation of the metal source back to the desired alignment.
- the orientation of the metal source being fed into the atomization zone may be monitored by a computerized monitoring system.
- the computerized system may capture images of the metal source relative to the plasma and/or the at least one plasma source.
- the system identifies when the metal source has spatially fluctuated so as to no longer being in its desired alignment.
- the computerized system can further determine an amount of the deviation and the correction required.
- the computer system can then issue a command to an alignment-correcting mechanism so as to adjust orientation of the metal source back to the desired alignment.
- the desired alignment may be alignment of the metal source fed into the atomization zone with an apex of the plasma jet from the at least one plasma source.
- the process can comprise aligning the heated metal source with the plasma of at least one plasma source comprises positioning the heated metal source within at most 5 centimeters from an outlet nozzle of the at least one plasma source.
- the process can comprise aligning the heated metal source with the plasma of at least one plasma source comprises positioning the heated metal source within at most 2.5 centimeters from an outlet nozzle of the at least one plasma source.
- the process can comprise aligning the heated metal source with the plasma of at least one plasma source comprises positioning the heated metal source within at most 1 .9 centimeters from an outlet nozzle of the at least one plasma source.
- the first atomizing system 2 includes a receptacle 8 that receives a feed of metal source 16 from an upstream system.
- the receptacle 8 may be a crucible.
- the metal source 16 within the receptacle 8 may be heated using various techniques known in the art, such as cooled-crucible technology (skull melting).
- heating of the metal source 16 within the receptacle 8 corresponds to heating of the metal source 16 prior to atomization.
- the metal source 16 is fed through an outlet 24 of the receptacle into the atomization zone 32.
- the heated metal source 16 exits through the outlet 24 under the forces of gravity.
- the heated metal source 16 exited from the receptacle 8 and fed into the atomization zone 32 is immediately contacted with plasma from at least one plasma source 40 that is also used to heat the high pressure cold gas that will produce a secondary atomization.
- the plasma source 40 includes at least one plasma torch. At least one angular nozzle 48 of the at least one plasma torch 40 is centered upon the metal source feed. For example, the cross- section of the nozzle 48 may be tapered towards the metal source feed so as to focus the plasma that contacts the metal source feed. As described elsewhere herein, the nozzle 48 may be positioned so that the apex of the plasma contacts the metal source fed from the receptacle 8. The contacting of the metal source feed by the plasma from the at least one plasma source 40 causes the metal source to be atomized.
- the nozzles of the torches are discrete nozzles 48 of the plasma torches that are oriented towards the metal source from the receptacle 8.
- the discrete nozzles 48 are positioned so that the apexes of the plasma outputted therefrom contacts the metal source from the receptacle 8.
- the atomizing system 2 further includes a gas source that feeds a secondary high pressure gas towards the atomization zone.
- the secondary gas flow contacts the pre-atomized metal source feed immediately after they have been formed from the plasma atomization.
- the gas source 56 can feed a high-pressure cold gas.
- the gas fed from the gas source 56 is an inert gas.
- Formed raw metal powder 64 is exited from the atomization zone 32.
- FIG. 2 therein illustrated is a schematic diagram of an adjustable guiding system 100 of an atomizing system according to various exemplary embodiments.
- the guiding system includes a guide 108 that defines a through channel.
- the guide 108 is positioned upstream of the atomization zone 32.
- the metal source that is received from an upstream system is fed into an inlet 1 16 of the guide 108.
- the metal source is then displaced through the channel of the guide 108.
- the metal source exits the guide 108 at an outlet 124 that is located in proximity of an atomization zone 32.
- the metal source 16 fed into the inlet 1 16 is in the form of a metal wire of a metal rod.
- the orientation of the guide 108 is adjustable. By adjusting the orientation of the guide 108, the orientation of the metal source 16 exited from the guide 108 and fed into the atomization zone 32 is also adjusted. Accordingly, the alignment of the metal source 16 fed into the atomization zone relative to the plasma source (not shown in Figure 2) may be adjusted via adjustments made to the guide 108.
- the guide 108 is pivotally coupled about a pivot point 132.
- the guide 108 may be coupled to a fixed portion of the atomizing system. By displacing an upper portion 140 of the guide 108, a lower portion 148 of guide 108 is displaced in a corresponding manner about the pivot point 132.
- the guiding system 100 further includes an alignment-correcting mechanism that is operable to displace the guide 108. Displacement of the guide 108 in turn displaces the metal source 16.
- the alignment-correcting mechanism comprises a displaceable member 156 that is coupled to an upper portion 140 of the guide 108.
- the displaceable member 156 is further coupled to at least one adjustor 164 that can cause displacement of the displaceable member 156.
- the adjustor 16 is an adjustment screw that is coupled to the displaceable member 156 via a threaded member 172. Turning of the adjustment screw 164 causes displacement of the threaded member 172, which further cause displacement of the displaceable member 156 and the guide 108.
- a plurality of differently oriented adjustors 16 may be provided to displace displaceable member 156 and the guide 108 in different directions.
- Arrows 174 denote possible directions of displacement of the guide member 108 within a plane.
- Arrows 176 denote possible displacement of the displaceable member 156 for causing displacement of the guide member 108 within a plane. It will be understood that the guide may be displaced in multiple directions.
- FIG. 3 therein illustrated is a cross-sectional view of a guide 108 according to one exemplary embodiment.
- the guide 108 defines a through channel 180 extending between its inlet 1 16 and outlet 124.
- An inner surface 188 of the through channel 180 may be lined with a material that does not contaminate the metal source 16 being displaced through the channel 180.
- the inner surface 188 of the through channel 180 may be formed of a heat-resistant material.
- the inner surface 188 of the through channel 180 may be formed of an electrically insulating material.
- the inner surface 188 is formed of a ceramic material.
- the ceramic material can be chosen from alumina oxyde, macor, zirconia, yttria, SiAION, silicium oxide and mixture thereof.
- the guide 108 may be formed of a heat-resistant material.
- the guide 108 may be formed of an electrically insulating material.
- the guide 108 may be formed of a ceramic material.
- the guide 108 includes cooling so as to cool the guide and restrict contamination of the metal source 16 being displaced through it.
- the guide 108 may have a cooling inlet 196 for receiving a cooling medium, such as a cooling gas or cooling liquid.
- the guide 108 is also double walled, wherein a cooling channel 204 is defined between an inner wall 212 and an outer wall 218.
- the cooling channel 204 is in fluid communication with the cooling inlet 196.
- the cooling channel 204 extends angularly about an axis of the guide 108 and also extends over a substantial portion of the length of the guide 108.
- Cooling medium exits via a cooling outlet 220 after having flowed through the cooling channel 204.
- the cooling of the guide 108 may be important according to exemplary embodiments wherein the metal source is already heated prior to entering the guide 108 and/or wherein the metal source is heated as it is displaced through the guide 108.
- the cooling inlet 196 is located downstream of the cooling outlet 220 along the path of displacement of the metal source 16 through the guide 108. Where the metal source 16 is heated, the metal source 16 at a downstream location, such as closer to the outlet 124, may be at a higher temperature than at an upstream location, such as the inlet 1 16. By positioning the inlet 196 downstream of the cooling outlet 220, cooling at a portion closer to the inlet 196 is prioritized.
- a lower end 228 of the guide 108 may be removable and replaceable. It will be appreciated that the lower end 228 is position within or in proximity of the atomization zone. Accordingly, the lower end 228 may be exposed to higher temperatures than other portions of the guide 108. This higher temperature may result in faster wear and tear of the lower end 228 than other portions of the guide 108, which can cause the lower end 228 to be replaced more often than the guide 108 itself.
- the metal source 16 may be heated as it is displaced through the guide 108.
- the heating element is a conductive coil 236 wound about a portion of the through channel 180.
- a current flowing through the conductive coil 236 produces a magnetic field, which further induces a current through the metal source 16 flowing through the channel 180.
- the induced current through the metal source 16 causes the metal source 16 to be heated.
- the metal source is heated via a form of inductive heating.
- the magnetic field produced by the conductive coil 236 does not induce a current through the inner surface 188 and/or guide 108 that can cause heating.
- FIG. 5 therein illustrated is a cross-sectional view of a guide having an electrode 244 for arc discharge heating.
- the guide 108 illustrated in Figure 5 does not have a cooling mechanism (cooling inlet 196, cooling channel 204 and cooling outlet 220).
- a cooling mechanism may also be included in the guide 108.
- the electrode 244 is placed in proximity of the metal source 16 as the source is exited from the outlet 124 of the guide 108.
- An electric arc 252 may be formed between the electrode 244 and the metal source 16, which causes heating of the metal source 16 by electric arc discharge.
- the metal source 16 may be further heated by resistive heating prior to be exited.
- a first probe may contact the metal source 16 upstream of the guide 108 or within the guide 108.
- a second probe may contact the metal source 16 downstream of the guide 108 as the electrode 244.
- An electrical power source connects the two probes, thereby forming an electrical circuit through the portion of the metal source 16 extending between the two probes. The current flowing through this portion of the metal source 16 causes it to be heated. It will be appreciated that the metal source is heated via resistive and arc discharge heating.
- FIG. 6 therein illustrated is a guided atomizing system 300 according to one exemplary embodiment.
- the metal source 16 extends through and is retained within a guide 108.
- the guide 108 is oriented so that the metal source 16 that is fed into the atomization zone 32 is appropriately aligned with the plasma jets 49 discharged from the nozzles 48 from the plasma sources 40.
- Arrows 174 denote exemplary freedom of movement of the guide 108 and metal source 16. However, it will be understood that the metal source 16 and guide 108 may also be displaced in other directions. The orientation of the guide 108 may be adjusted to maintain proper alignment of the metal source 16 fed into the atomization zone with the plasma from the plasma source 40 and/or the nozzle 48 of the plasma source.
- the illustrated example shows the plasma source 40 as being plasma torches with discrete nozzles.
- the plasma source 40 may emit plasma from an annular nozzle.
- the atomizing system 300 includes a conductive coil 236 for induction heating of the metal source 16 as it is displaced through the guide 108.
- the atomizing system 300 may further include a gas recovering system 316 which recovers the gas present within a collection chamber 324 downstream of the atomization zone 32. The recovered gas may be fed back into the atomization zone 32 as atomizing gas for the formed raw metal powders. Raw metal powders produced by the atomizing system 300 may be further collected within the atomizing system 300.
- guided atomizing system 300 includes an electrode 244 positioned in proximity of the atomization zone 300.
- the electrode 244 forms an electric arc with the metal source 16, which causes a current to flow through the metal source 16 to heat it.
- an electrical power source 324 is provided to provide the current flow and create the electric arc.
- the guided atomizing system 300 includes both a conductive coil 236 for causing induction heating of the metal source 16 and an electrode 244 for causing arc discharging heating of the metal source.
- the heated melt source can comprise at least one member chosen from titanium, titanium alloys, zirconium, zirconium alloys, cobalt superalloys, nickel superalloys, magnesium, magnesium alloys, niobium, niobium alloys, aluminum, aluminum alloys, molybdenum, molybdenum alloys, tungsten, tungsten alloys, oxygen-reactive metals, and nitrogen-reactive metals.
- the melt source can be chosen from titanium, titanium alloys, zirconium, zirconium alloys, cobalt superalloys, nickel superalloys, magnesium, magnesium alloys, niobium, niobium alloys, aluminum, aluminum alloys, molybdenum, molybdenum alloys, tungsten, tungsten alloys, oxygen-reactive metals, and nitrogen-reactive metals.
- the melt source can be chosen from titanium, titanium alloys, zirconium, zirconium alloys, aluminum and aluminum alloys.
- the melt source can be chosen from titanium alloys.
- the melt source can be a titanium alloy.
- the titanium alloy can be chosen from Ti-6A-4V, ⁇ -6 ⁇ - 2Sn-4Zr-2Mo, Ti-5AI-5V-5Mo-3Cr, and titanium aluminides.
- the melt source can be chosen from unalloyed Ti Grades (for example grade 1 , 2, 3 or 4); Ti alloys modified with Pd or Ru (for example grade 7, 1 1 , 16, 17, 26 or 27); alpha and near-alpha Ti alloys (for example grade 6, 9, 12, 18, 28; alpha-beta Ti alloys (for example grade 5, 23 or 29); near-beta and beta Ti alloys (for example grade 19 or 20).
- unalloyed Ti Grades for example grade 1 , 2, 3 or 4
- Ti alloys modified with Pd or Ru for example grade 7, 1 1 , 16, 17, 26 or 27
- alpha and near-alpha Ti alloys for example grade 6, 9, 12, 18, 28
- alpha-beta Ti alloys for example grade 5, 23 or 29
- near-beta and beta Ti alloys for example grade 19 or 20.
- plasma atomization can be carried out with various types of plasma torches such as DC plasma torches, AC plasma torches, RF plasma torches, microwave plasma torches or 3 phases plasma arc torches.
- plasma torches such as DC plasma torches, AC plasma torches, RF plasma torches, microwave plasma torches or 3 phases plasma arc torches.
- a plasma atomization run is achieved using a 0.125" diameter wire of Ti-6AI-4V (gr. 23) as raw material and 3 converging plasma jets oriented at about 30° with respect to the vertical axis.
- the plasma contacts the metal wire at a location that is within less than 2.5 centimeters of the plasma torch nozzle outlet.
- Each plasma torch is operated at a power of 30 kW with a 150 SLM argon gas flow.
- a background sheath gas is also used to ensure proper transport of metal droplets.
- the sheath gas flow is at 550 SLM.
- a dc electric current varying from 150 A to 180 A at an electric potential of 45 V is used to preheat the wire at elevated temperature prior to the atomization with the plasma jets and it results in a wire feed rate varying from 8 to 13 kg/h.
- the wire is fed through a gas cooled and adjustable guide to enable a continuous metal feeding right to the apex of the plasma torch jets.
- the batch size is typically of 100 kg for each run.
- the particle size distribution obtained is determined according to ASTM B214.
- a first batch (batch 1 ) was produced using a gas-to-metal ration of 8.7 and a plasma outlet to atomization zone (location of contact between plasma and metal source) of about 2.5 centimeters.
- a second batch (batch 2) was produced using a gas-to-metal ratio of 12.9 and a plasma outlet to atomization zone (location of contact between plasma and metal source) of about 1 .9 centimeters. [00132] The yield results for the batch 1 and 2
- the powder produced is very pure and spherical and contains a large fraction of fine powder that can be used in applications such laser additive manufacturing and powder injection molding.
- Figure 9 is a scanning electron microscopy (SEM) image at 250 times magnification of the as-is raw metal powders formed (without sieving) within the example process.
- Figure 10 is a SEM image at 500 times magnification of the as-is raw metal powders formed (without sieving) within the example process.
- Figure 1 1 is a SEM image at 2000 times magnification of as-is raw metal powders formed (without sieving) within the example process.
- a plasma atomization run is achieved using a 0.125" diameter wire of Ti-6AI-2Sn-4Zr-2Mo-0.08Si as raw material and 3 converging plasma jets oriented at about 30° with respect to the vertical axis.
- the plasma contacts the metal wire at a location that is within less than 2.0 centimeters of the plasma torch nozzle outlet.
- Each plasma torch is operated at a power of 30 kW with a 150 SLM argon gas flow.
- a background sheath gas is also used to ensure proper transport of metal droplets.
- the sheath gas flow is at 550 SLM.
- a dc electric current of 150A at an electric potential of 45 V is used to preheat the wire at elevated temperature prior to the atomization with the plasma jets and it results in a wire feed rate of 8.5 kg/h.
- the wire is fed through a gas cooled and adjustable guide to enable a continuous metal feeding right to the apex of the plasma torch jets.
- the batch size is typically of 100 kg for the run.
- Molybdenum range 1.93 ASTM E 2371 - Direct current plasma emission spectroscopy
- a plasma atomization run is achieved using a 0.080" diameter wire of zirconium as raw material and 3 converging plasma jets oriented at about 30° with respect to the vertical axis.
- the plasma contacts the metal wire at a location that is within less than 2.0 centimeters of the plasma torch nozzle outlet.
- Each plasma torch is operated at a power of 30 kW with a 150 SLM argon gas flow.
- a background sheath gas is also used to ensure proper transport of metal droplets.
- the sheath gas flow is at 550 SLM.
- a dc electric current of 1 15 A at an electric potential of 45 V is used to preheat the wire at elevated temperature prior to the atomization with the plasma jets and it results in a wire feed rate of 6.0 kg/h.
- the wire is fed through a gas cooled and adjustable guide to enable a continuous metal feeding right to the apex of the plasma torch jets.
- the batch size is typically of 50 kg for the run.
- Chromium range 0.11 ASTM E1097
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